CN109824276A - A kind of phosphorus doping self-cleaning list silver LOW-E glass and preparation method thereof - Google Patents
A kind of phosphorus doping self-cleaning list silver LOW-E glass and preparation method thereof Download PDFInfo
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Abstract
This application discloses a kind of phosphorus doping self-cleaning list silver LOW-E glass and preparation method thereof, by on glass matrix lateral surface, as self-cleaning film, while on glass matrix medial surface, successively plating sets the first Si to phosphors coating titania coextruded film layer to the phosphorus doping self-cleaning list silver LOW-E glass of the application3N4Film layer, AZO film layer, Ag film layer, NiCr film layer, the 2nd Si3N4Film layer is as low radiation composite film, it may be implemented in 380~780nm of visible wavelength range response, improve the transmissivity and sunlight transmittance of visible light, make the phosphorus doping self-cleaning list silver LOW-E glass that there is excellent energy-saving effect, there is visible light-responded self-cleaning net effect simultaneously, a kind of preparation method of phosphorus doping self-cleaning list silver LOW-E glass of the application has the advantages that the adhesive force of high deposition rate, film layer and substrate is strong, reproducible, at low cost.
Description
[technical field]
The application belongs to glassmaking art, and in particular to a kind of phosphorus doping self-cleaning list silver LOW-E glass and its
Preparation method.
[background technique]
Low emissivity glass, also known as LOW-E glass, it is after the oxidation film that glass surface plates silverskin or fluorine doped, in utilization
The property for stating film layer reflecting far-infrared ray achievees the purpose that heat-insulated, heat preservation, is divided into single silver low radiation film tying by film structure
Structure and double silver low radiation film structures, are increasingly used in many utilities buildings especially skyscraper.However, Low emissivity plates
Film glass is relatively difficult with certain risk as the glass curtain wall progress high-altitude cleaning of building, and therefore, people are low
Radiant glass surface coated with nano TiO2Film utilizes TiO2There is mechanism of degradation object, makes low emissivity glass surface in sunlight
The ability of the lower organic pollutant that its surface is attached to degradation, enables the organic dust for being attached to its surface to be easy to by water
It washes.
But pure TiO2In the crystalline state of film, it is brilliant to show tetragonal crystal system anatase in the cubic shape of rule for crystal grain
Pattern, do not have 380~780nm of visible wavelength range response, so that self-cleaning net effect is general, cause to meet and too yet
The decline of sunlight transmissivity, seriously affects the energy-saving effect of low emissivity glass.
[summary of the invention]
In order to solve the above-mentioned technical problem the application, provides a kind of phosphorus doping self-cleaning list silver LOW-E glass, having can
The self-cleaning net effect of light-exposed 380~780nm of wave-length coverage response not only has excellent energy-saving effect, also have it is good from
Clean effect.
It is a further object of the present invention to provide a kind of preparation methods of phosphorus doping self-cleaning list silver LOW-E glass.
In order to solve the above technical problems, the application uses following technical scheme:
A kind of phosphorus doping self-cleaning list silver LOW-E glass, including the first glass substrate, the second glass matrix and be set to two
Hollow sealing chamber between person, first glass substrate include the first glass matrix, be set to first glass matrix it is separate
Phosphorus titania coextruded film layer in the hollow sealing Cavity surface and successively plating are set to first glass matrix close to institute
State the first Si in hollow sealing Cavity surface3N4Film layer, AZO film layer, Ag film layer, NiCr film layer, the 2nd Si3N4Film layer.
A kind of phosphorus doping self-cleaning list silver LOW-E glass as described above, the phosphorus titania coextruded film tunic are thick
90~110nm.
A kind of phosphorus doping self-cleaning list silver LOW-E glass as described above, the first Si3N420~45nm of film layer film thickness.
A kind of phosphorus doping self-cleaning list silver LOW-E glass as described above, 8~10nm of the Ag film layer film thickness.
A kind of phosphorus doping self-cleaning list silver LOW-E glass as described above, 3~5nm of the NiCr film layer film thickness.
A kind of phosphorus doping self-cleaning list silver LOW-E glass as described above, the 2nd Si3N450~85nm of film layer film thickness.
A kind of preparation method of phosphorus doping self-cleaning list silver LOW-E glass, comprising the following steps:
A, phosphors coating titania coextruded film layer: with rolling method by 5% p-doped TiO2Solution is coated to 4~10mm of thickness
Any side surface of the first glass matrix on, coating film thickness be 90~110nm phosphorus titania coextruded film layer, put after coating
Enter tempering in annealing furnace, obtains the self-cleaning glass of tempering；
B, above-mentioned self-cleaning glass is not coated with clad can cleaning, is sent into magnetron sputtering machine after cleaning and successively carries out magnetic control
Sputtering；
C, plating sets the first Si3N4Film layer: being sputtered with AC power source, Ar, N2As sputter gas, magnetron sputtering sial target Si:
Al=92:8 (wt%), Ar, N2Gas flow 400SCCM:600SCCM, magnetron-sputtered film thickness are the first Si of 20~45nm3N4
Film layer；
D, plating sets AZO film layer: being sputtered with AC power source, Ar, O2As sputter gas, magnetron sputtering Al-Doped ZnO target
ZnO:Al=92:8 (wt%), Ar, O2Gas flow 1000SCCM:40SCCM, magnetron-sputtered film thickness are the AZO of 300~500nm
Film layer；
E, plating sets Ag film layer: being sputtered with DC power supply, Ar is as sputter gas, 500~550SCCM of gas flow, magnetic control
Sputter the Ag film layer that film thickness is 8~10nm；
F, plating sets NiCr film layer: being sputtered with DC power supply, Ar is as sputter gas, 500~550SCCM of gas flow, magnetic
The NiCr film layer that control sputtering film thickness is 3~5nm；
G, plating sets the 2nd Si3N4Film layer: being sputtered with AC power source, Ar, N2As sputter gas, magnetron sputtering sial target Si:
Al=92:8 (wt%), Ar, N2Gas flow 400SCCM:600SCCM, magnetron-sputtered film thickness are the 2nd Si of 50~85nm3N4
Film layer obtains single layer phosphorus doping self-cleaning list silver LOW-E glass；
H, the single layer phosphorus doping self-cleaning list silver LOW-E glass plating processing synthesis: is equipped with the first Si3N4Film layer,
The AZO film layer, the Ag film layer, the NiCr film layer, the 2nd Si3N4The one side of film layer, with 4~10mm of thickness
Two glass matrix, which are separated out after hollow sealing chamber, to carry out processing synthesis and becomes hollow glass, both.
A kind of preparation method of phosphorus doping self-cleaning list silver LOW-E glass as described above, 5% p-doped described in step A
TiO2The preparation method of solution includes the following steps:
A, 30~100ml butyl titanate is dissolved in 190~210ml dehydrated alcohol, 20~30mlH2O2In, stirring 20~
40min instills 30~50ml deionized water while stirring, obtains the first mixed solution；
B, 10~20ml acetylacetone,2,4-pentanedione, 20~30mlHNO are added in above-mentioned first mixed solution3, it is heated to 30~50
DEG C, 20~40min is stirred, the second mixed solution is obtained；
C, 6~20mlH is instilled in above-mentioned second mixed solution3PO4, 70~90 DEG C are heated to, 1.5~2.5h is stirred, obtains
Third mixed solution；
D, above-mentioned third mixed solution is put into the stainless steel autoclave with polytetrafluoroethyllining lining, is heated to 130
~140 DEG C, 3~4bar of pressure, stir 1.5~2.5h after filtering to get.
Compared with prior art, the application has the beneficial effect that:
The invention discloses a kind of phosphorus doping self-cleaning list silver LOW-E glass, by coating on glass matrix lateral surface
As self-cleaning film, while on glass matrix medial surface, successively plating sets the first Si to phosphorus titania coextruded film layer3N4Film layer,
AZO film layer, Ag film layer, NiCr film layer, the 2nd Si3N4Film layer is as low radiation composite film, it can be achieved that in visible wavelength range
380~780nm response, improves the transmissivity and sunlight transmittance of visible light, makes the phosphorus doping self-cleaning list silver LOW-E glass
Glass has excellent energy-saving effect, while having visible light-responded self-cleaning net effect；Through the embodiment of the present application test result table
It is bright, the application phosphorus doping TiO2The transmission of visible light ﹥ 68% of low emissivity glass obtained, infrared transmittivity ﹤ 19%, heat transfer system
Number ﹤ 1.68 [W/ (㎡ K)], shading coefficient ﹤ 0.48, radiance ﹤ 0.086, testing result are superior to pure TiO2It is obtained low
Radiant glass, with high visible light transmissivity, low-E, low infrared transmittivity, low heat transfer coefficient and low shading coefficient
Feature allows visible light well to penetrate the incoming interior of glass, enhances daylighting effect, while stopping from the outdoor hot spoke of far infrared
It penetrates, plays insulation effect, save resource, energy-saving and environment-friendly effect；Hydrophily is the important indicator of self-cleaning glass, passes through contact
Angle can intuitively reflect the quality of self-cleaning net effect, the application p-doped TiO2Obtained low emissivity glass, 4.9 ° of contact angle ﹤,
And pure TiO2Obtained low emissivity glass, contact angle is 8.4 ° and 8.6 °, it can thus be appreciated that the application has more preferable self-cleaning
Effect has the self-cleaning net effect responded in 380~780nm of visible wavelength range, can reduce cladding glass wash number, this
Application has a wide range of applications scene in glass curtain wall, building doors and windows.
A kind of preparation method of phosphorus doping self-cleaning list silver LOW-E glass of the invention, phosphorus titania coextruded film layer
By coating 5% p-doped TiO with rolling method2Tempering after solution and obtain, the first Si of low radiation composite film3N4Film layer, AZO film layer, Ag
Film layer, NiCr film layer, the 2nd Si3N4Film layer through magnetron sputtering method on the glass surface magnetron sputtering and obtain, 5% p-doped
TiO2Solution is to make predecessor, dehydrated alcohol, the 20~30mlH of 190~210ml using the butyl titanate of 30~100ml2O2、
30~50ml deionization water as solvent, the acetylacetone,2,4-pentanedione of 10~20ml make chelating agent, the HNO of 20~30ml3Make catalyst, then plus
Enter the H of 6~20ml3PO4It is made, the TiO after phosphorus doping is obtained by Optimization2Film makes TiO2The crystal shape of film is sent out
Raw apparent variation, may occur in which the anatase crystalline form of cylindrical directional profile, it can be achieved that visible wavelength range 380~
780nm response, improves the transmissivity and sunlight transmittance of visible light, has the phosphorus doping self-cleaning list silver LOW-E glass
The preparation method for having excellent energy-saving effect, while having visible light-responded self-cleaning net effect, and invent has deposition rate
Strong, reproducible, the at low cost advantage of the adhesive force of high, film layer and substrate.
[Detailed description of the invention]
In order to more clearly explain the technical solutions in the embodiments of the present application, make required in being described below to embodiment
Attached drawing is briefly described.
Fig. 1 is a kind of structural schematic diagram of phosphorus doping self-cleaning list silver LOW-E glass of the present invention.
[specific embodiment]
A kind of phosphorus doping self-cleaning list silver LOW-E glass as described in Figure 1, including the first glass substrate 1, the second glass base
Body 2 and set on hollow sealing chamber 3 between the two.First glass substrate 1 includes the first glass matrix 11, set on described
First glass matrix 11 is plated far from the phosphorus titania coextruded film layer 12 on 3 face of hollow sealing chamber and successively is set to institute
State first Si of first glass matrix 11 on 3 face of hollow sealing chamber3N4Film layer 13, AZO film layer 14, Ag film layer 15,
NiCr film layer 16, the 2nd Si3N4Film layer 17.
The application on 11 lateral surface of glass matrix by coating the phosphorus titania coextruded film layer 12 as self-cleaning
Net film, while successively plating sets the first Si on 11 medial surface of glass matrix3N4Film layer 13, the AZO film layer 14, the Ag
Film layer 15, the NiCr film layer 16, the 2nd Si3N4Film layer 17 is as low radiation composite film, it can be achieved that in visible wavelength model
380~780nm response is enclosed, the transmissivity and sunlight transmittance of visible light is improved, makes the phosphorus doping self-cleaning list silver LOW-E
Glass has excellent energy-saving effect, while having visible light-responded self-cleaning net effect.The phosphorus doping of the application is self-cleaning
Net single silver LOW-E glass has high visible light transmissivity, low-E, low infrared transmittivity, low heat transfer coefficient and low sunshade
The characteristics of coefficient, permission visible light well penetrate the incoming interior of glass, enhance daylighting effect, while stopping from the remote red of outdoor
Outer heat radiation has the self-cleaning net effect responded in 380~780nm of visible wavelength range, can reduce cladding glass cleaning time
Number.
12 90~the 110nm of film thickness of phosphorus titania coextruded film layer, to coat 5% p-doped TiO with rolling method2Solution
Afterwards tempering and obtain, the 5% p-doped TiO2Solution is to make predecessor, 190~210ml using the butyl titanate of 30~100ml
Dehydrated alcohol, 20~30mlH2O2, 30~50ml deionization water as solvent, the acetylacetone,2,4-pentanedione of 10~20ml makees chelating agent, 20~
The HNO of 30ml3Make catalyst, adds the H of 6~20ml3PO4It is made.Due to pure TiO2In the crystalline state of film, crystal grain
In regular cubic shape, the pattern of tetragonal crystal system anatase crystalline substance is shown, does not have 380~780nm of visible wavelength range response,
And the phosphorus titania coextruded film layer 12 of the application, the TiO after phosphorus doping is obtained by Optimization2Film makes TiO2Film
Crystal shape apparent variation occurs, may occur in which the anatase crystalline form of cylindrical directional profile, it can be achieved that in visible light wave
Long 380~780nm of range response, improves the transmissivity and sunlight transmittance of visible light, makes the phosphorus doping self-cleaning Dan Yin
LOW-E glass has excellent energy-saving effect, while having visible light-responded self-cleaning net effect.The phosphorus titanium dioxide of the application
Composite film layer 12 has Superhydrophilic, and hydrophily is the important indicator of self-cleaning net effect, by hydrophily feature, makes described
Phosphorus doping self-cleaning list silver LOW-E glass can make water be easy to sprawl on the surface, so that dust etc. be made to be adsorbed on glass table
The inorganic matter in face can be easily flushed away, and natural rainwater can make self-cleaning glass keep permanent clean under normal circumstances
Only.
First Si3N413 20~45nm of film thickness of film layer is magnetron sputtering sial target Si:Al=92:8 (wt%), exchange
Power supply sputtering, with Ar, N2As sputter gas, Ar, N2Gas flow 400SCCM:600SCCM.First Si3N4Film layer 13
As first medium film layer, firmness with higher improves the low-radiation film 13 and first glass matrix 11
Adhesive force, while to infrared ray have high reflectance, the phosphorus doping self-cleaning list silver LOW-E glass can be increased to infrared waves
The reflectivity of section.
14 300~the 500nm of film thickness of AZO film layer is magnetron sputtering Al-Doped ZnO target ZnO:Al=92:8 (wt%),
AC power source sputtering, with Ar, O2Gas flow 1000SCCM:40SCCM.The AZO film layer 14 is the zinc oxide films of aluminium doping
Film, effect are to reduce infrared transmitance.
15 8~the 10nm of film thickness of Ag film layer, is magnetron sputtering Ag film layer, and DC power supply sputtering uses Ar as sputtering gas
Body, 500~550SCCM of gas flow.The Ag film layer 15 is used as functional film layer, and effect is reflection infrared ray, reduces simultaneously
The ultraviolet light of destructive effects enters the room in sunlight.
16 3~the 5nm of film thickness of NiCr film layer, is magnetron sputtering NiCr film layer, and DC power supply sputtering uses Ar as sputtering
Gas, 500~550SCCM of gas flow.The NiCr film layer functions as masking film layer, and effect is to prevent Ag film layer
15 aoxidize and lose low radiation functions.
2nd Si3N417 50~85nm of film thickness of film layer is magnetron sputtering sial target Si:Al=92:8 (wt%), exchange
Power supply sputtering, with Ar, N2As sputter gas, Ar, N2Gas flow 400SCCM:600SCCM.As theca externa media coating,
The film layer has high reflectance, while the Si to infrared ray3N4Film layer 17 has good hardness, can protect the Ag very well
Film layer 15 improves the physical and chemical performance of the phosphorus doping self-cleaning list silver LOW-E glass.
First glass matrix 11 and second glass matrix 2 are the float glass of 4~10mm of thickness, use float glass process
Glass has preferable translucency and lighting performance as glass matrix.By by first glass matrix 11 and described the
The processing of two glass matrix 2 synthesizes hollow glass, and the phosphorus titania coextruded film layer 12 is coated to first glass
11 lateral surface of matrix, the low radiation composite film 13 plating are located at the first glass matrix 11 towards on the face of the hollow sealing chamber 3, right
The low radiation composite film 13 is protected, and prevents from aoxidizing and destroying, hollow glass inherently has energy-saving effect, added low
The energy-saving effect for radiating film, can make the energy-saving effect of whole building glass more preferable, on the other hand can use hollow glass sound insulation
Performance reduces noise pollution.
The application on 11 lateral surface of glass matrix by coating the phosphorus titania coextruded film layer 12 as self-cleaning
Net film, while successively plating sets the first Si on glass matrix medial surface3N4Film layer 13, the AZO film layer 14, the Ag film
Layer 15, the NiCr film layer 16, the 2nd Si3N4Film layer 17 is as low radiation composite film, it can be achieved that in visible wavelength range
380~780nm response, improves the transmissivity and sunlight transmittance of visible light, makes the phosphorus doping self-cleaning list silver LOW-E glass
Glass has excellent energy-saving effect, while having visible light-responded self-cleaning net effect.
The preparation side of 1~6 pair of a kind of phosphorus doping self-cleaning list silver LOW-E glass of the invention combined with specific embodiments below
Method is further described:
Embodiment 1:
A kind of preparation method of phosphorus doping self-cleaning list silver LOW-E glass the following steps are included:
A, phosphors coating titania coextruded film layer: with rolling method by 5% p-doped TiO2Solution is coated to the of thickness 6mm
On any side surface of one glass matrix, the phosphorus titania coextruded film layer that coating film thickness is 100nm is put into annealing furnace after coating
Middle tempering obtains the self-cleaning glass of tempering；
B, above-mentioned self-cleaning glass is not coated with clad can cleaning, is sent into magnetron sputtering machine after cleaning and successively carries out magnetic control
Sputtering；
C, plating sets the first Si3N4Film layer: being sputtered with AC power source, Ar, N2As sputter gas, magnetron sputtering sial target Si:
Al=92:8 (wt%), Ar, N2Gas flow 400SCCM:600SCCM, magnetron-sputtered film thickness are the first Si of 30nm3N4Film layer；
D, plating sets AZO film layer: being sputtered with AC power source, Ar, O2As sputter gas, magnetron sputtering Al-Doped ZnO target
ZnO:Al=92:8 (wt%), Ar, O2Gas flow 1000SCCM:40SCCM, magnetron-sputtered film thickness are the AZO film layer of 400nm；
E, plating sets Ag film layer: being sputtered with DC power supply, Ar is as sputter gas, gas flow 500SCCM, magnetron sputtering film
Thickness is the Ag film layer of 10nm；
F, plating sets NiCr film layer: being sputtered with DC power supply, Ar is as sputter gas, gas flow 520SCCM, magnetron sputtering
Film thickness is the NiCr film layer of 4nm；
G, plating sets the 2nd Si3N4Film layer: being sputtered with AC power source, Ar, N2As sputter gas, magnetron sputtering sial target Si:
Al=92:8 (wt%), Ar, N2Gas flow 400SCCM:600SCCM, magnetron-sputtered film thickness are the 2nd Si of 60nm3N4Film layer,
Obtain single layer phosphorus doping self-cleaning list silver LOW-E glass；
H, the single layer phosphorus doping self-cleaning list silver LOW-E glass plating processing synthesis: is equipped with the first Si3N4Film layer,
The AZO film layer, the Ag film layer, the NiCr film layer, the 2nd Si3N4The one side of film layer, the second glass with thickness 6mm
Glass matrix, which is separated out after hollow sealing chamber, to carry out processing synthesis and becomes hollow glass, both.
5% p-doped TiO described in above-mentioned steps A2The preparation method of solution includes the following steps:
A, 70ml butyl titanate is dissolved in 200ml dehydrated alcohol, 25mlH2O2In, 30min is stirred, is instilled while stirring
40ml deionized water obtains the first mixed solution；
B, 15ml acetylacetone,2,4-pentanedione, 25mlHNO are added in above-mentioned first mixed solution3, 40 DEG C are heated to, 30min is stirred,
Obtain the second mixed solution；
C, 14mlH is instilled in above-mentioned second mixed solution3PO4, 80 DEG C are heated to, 2.0h is stirred, it is molten to obtain third mixing
Liquid；
D, above-mentioned third mixed solution is put into the stainless steel autoclave with polytetrafluoroethyllining lining, is heated to 135
DEG C, pressure 4bar, stir 2.0h after filtering to get.
Embodiment 2:
A kind of preparation method of phosphorus doping self-cleaning list silver LOW-E glass the following steps are included:
A, phosphors coating titania coextruded film layer: with rolling method by 5% p-doped TiO2Solution is coated to the of thickness 4mm
On any side surface of one glass matrix, the phosphorus titania coextruded film layer that coating film thickness is 110nm is put into annealing furnace after coating
Middle tempering obtains the self-cleaning glass of tempering；
B, above-mentioned self-cleaning glass is not coated with clad can cleaning, is sent into magnetron sputtering machine after cleaning and successively carries out magnetic control
Sputtering；
C, plating sets the first Si3N4Film layer: being sputtered with AC power source, Ar, N2As sputter gas, magnetron sputtering sial target Si:
Al=92:8 (wt%), Ar, N2Gas flow 400SCCM:600SCCM, magnetron-sputtered film thickness are the first Si of 25nm3N4Film layer；
D, plating sets AZO film layer: being sputtered with AC power source, Ar, O2As sputter gas, magnetron sputtering Al-Doped ZnO target
ZnO:Al=92:8 (wt%), Ar, O2Gas flow 1000SCCM:40SCCM, magnetron-sputtered film thickness are the AZO film layer of 300nm；
E, plating sets Ag film layer: being sputtered with DC power supply, Ar is as sputter gas, gas flow 530SCCM, magnetron sputtering film
Thickness is the Ag film layer of 10nm；
F, plating sets NiCr film layer: being sputtered with DC power supply, Ar is as sputter gas, gas flow 510SCCM, magnetron sputtering
Film thickness is the NiCr film layer of 3nm；
G, plating sets the 2nd Si3N4Film layer: being sputtered with AC power source, Ar, N2As sputter gas, magnetron sputtering sial target Si:
Al=92:8 (wt%), Ar, N2Gas flow 400SCCM:600SCCM, magnetron-sputtered film thickness are the 2nd Si of 80nm3N4Film layer,
Obtain single layer phosphorus doping self-cleaning list silver LOW-E glass；
H, the single layer phosphorus doping self-cleaning list silver LOW-E glass plating processing synthesis: is equipped with the first Si3N4Film layer,
The AZO film layer, the Ag film layer, the NiCr film layer, the 2nd Si3N4The one side of film layer, the second glass with thickness 8mm
Glass matrix, which is separated out after hollow sealing chamber, to carry out processing synthesis and becomes hollow glass, both.
5% p-doped TiO described in above-mentioned steps A2The preparation method of solution includes the following steps:
A, 85ml butyl titanate is dissolved in 195ml dehydrated alcohol, 20mlH2O2In, 35min is stirred, is instilled while stirring
50ml deionized water obtains the first mixed solution；
B, 10ml acetylacetone,2,4-pentanedione, 30mlHNO are added in above-mentioned first mixed solution3, 30 DEG C are heated to, 40min is stirred,
Obtain the second mixed solution；
C, 8mlH is instilled in above-mentioned second mixed solution3PO4, 90 DEG C are heated to, 2.2h is stirred, obtains third mixed solution；
D, above-mentioned third mixed solution is put into the stainless steel autoclave with polytetrafluoroethyllining lining, is heated to 133
DEG C, pressure 3bar, stir 2.0h after filtering to get.
Embodiment 3:
A kind of preparation method of phosphorus doping self-cleaning list silver LOW-E glass the following steps are included:
A, phosphors coating titania coextruded film layer: with rolling method by 5% p-doped TiO2Solution is coated to thickness 10mm's
On any side surface of first glass matrix, the phosphorus titania coextruded film layer that coating film thickness is 90nm is put into tempering after coating
Tempering in furnace obtains the self-cleaning glass of tempering；
B, above-mentioned self-cleaning glass is not coated with clad can cleaning, is sent into magnetron sputtering machine after cleaning and successively carries out magnetic control
Sputtering；
C, plating sets the first Si3N4Film layer: being sputtered with AC power source, Ar, N2As sputter gas, magnetron sputtering sial target Si:
Al=92:8 (wt%), Ar, N2Gas flow 400SCCM:600SCCM, magnetron-sputtered film thickness are the first Si of 45nm3N4Film layer；
D, plating sets AZO film layer: being sputtered with AC power source, Ar, O2As sputter gas, magnetron sputtering Al-Doped ZnO target
ZnO:Al=92:8 (wt%), Ar, O2Gas flow 1000SCCM:40SCCM, magnetron-sputtered film thickness are the AZO film layer of 500nm；
E, plating sets Ag film layer: being sputtered with DC power supply, Ar is as sputter gas, gas flow 510SCCM, magnetron sputtering film
Thickness is the Ag film layer of 8nm；
F, plating sets NiCr film layer: being sputtered with DC power supply, Ar is as sputter gas, gas flow 550SCCM, magnetron sputtering
Film thickness is the NiCr film layer of 3.5nm；
G, plating sets the 2nd Si3N4Film layer: being sputtered with AC power source, Ar, N2As sputter gas, magnetron sputtering sial target Si:
Al=92:8 (wt%), Ar, N2Gas flow 400SCCM:600SCCM, magnetron-sputtered film thickness are the 2nd Si of 75nm3N4Film layer,
Obtain single layer phosphorus doping self-cleaning list silver LOW-E glass；
H, the single layer phosphorus doping self-cleaning list silver LOW-E glass plating processing synthesis: is equipped with the first Si3N4Film layer,
The AZO film layer, the Ag film layer, the NiCr film layer, the 2nd Si3N4The one side of film layer, the second glass with thickness 6mm
Glass matrix, which is separated out after hollow sealing chamber, to carry out processing synthesis and becomes hollow glass, both.
5% p-doped TiO described in above-mentioned steps A2The preparation method of solution includes the following steps:
A, 100ml butyl titanate is dissolved in 190ml dehydrated alcohol, 30mlH2O2In, 40min is stirred, is instilled while stirring
35ml deionized water obtains the first mixed solution；
B, 12ml acetylacetone,2,4-pentanedione, 28mlHNO are added in above-mentioned first mixed solution3, 35 DEG C are heated to, 35min is stirred,
Obtain the second mixed solution；
C, 18mlH is instilled in above-mentioned second mixed solution3PO4, 85 DEG C are heated to, 2.5h is stirred, it is molten to obtain third mixing
Liquid；
D, above-mentioned third mixed solution is put into the stainless steel autoclave with polytetrafluoroethyllining lining, is heated to 130
DEG C, pressure 3.5bar, stir 1.5h after filtering to get.
Embodiment 4:
A kind of preparation method of phosphorus doping self-cleaning list silver LOW-E glass the following steps are included:
A, phosphors coating titania coextruded film layer: with rolling method by 5% p-doped TiO2Solution is coated to the of thickness 6mm
On any side surface of one glass matrix, the phosphorus titania coextruded film layer that coating film thickness is 105nm is put into annealing furnace after coating
Middle tempering obtains the self-cleaning glass of tempering；
B, above-mentioned self-cleaning glass is not coated with clad can cleaning, is sent into magnetron sputtering machine after cleaning and successively carries out magnetic control
Sputtering；
C, plating sets the first Si3N4Film layer: being sputtered with AC power source, Ar, N2As sputter gas, magnetron sputtering sial target Si:
Al=92:8 (wt%), Ar, N2Gas flow 400SCCM:600SCCM, magnetron-sputtered film thickness are the first Si of 40nm3N4Film layer；
D, plating sets AZO film layer: being sputtered with AC power source, Ar, O2As sputter gas, magnetron sputtering Al-Doped ZnO target
ZnO:Al=92:8 (wt%), Ar, O2Gas flow 1000SCCM:40SCCM, magnetron-sputtered film thickness are the AZO film layer of 350nm；
E, plating sets Ag film layer: being sputtered with DC power supply, Ar is as sputter gas, gas flow 550SCCM, magnetron sputtering film
Thickness is the Ag film layer of 9nm；
F, plating sets NiCr film layer: being sputtered with DC power supply, Ar is as sputter gas, gas flow 530SCCM, magnetron sputtering
Film thickness is the NiCr film layer of 4.5nm；
G, plating sets the 2nd Si3N4Film layer: being sputtered with AC power source, Ar, N2As sputter gas, magnetron sputtering sial target Si:
Al=92:8 (wt%), Ar, N2Gas flow 400SCCM:600SCCM, magnetron-sputtered film thickness are the 2nd Si of 85nm3N4Film layer,
Obtain single layer phosphorus doping self-cleaning list silver LOW-E glass；
H, the single layer phosphorus doping self-cleaning list silver LOW-E glass plating processing synthesis: is equipped with the first Si3N4Film layer,
The AZO film layer, the Ag film layer, the NiCr film layer, the 2nd Si3N4The one side of film layer, the second glass with thickness 4mm
Glass matrix, which is separated out after hollow sealing chamber, to carry out processing synthesis and becomes hollow glass, both.
5% p-doped TiO described in above-mentioned steps A2The preparation method of solution includes the following steps:
A, 30ml butyl titanate is dissolved in 250ml dehydrated alcohol, 28mlH2O2In, 20min is stirred, is instilled while stirring
30ml deionized water obtains the first mixed solution；
B, 18ml acetylacetone,2,4-pentanedione, 22mlHNO are added in above-mentioned first mixed solution3, 45 DEG C are heated to, 20min is stirred,
Obtain the second mixed solution；
C, 20mlH is instilled in above-mentioned second mixed solution3PO4, 80 DEG C are heated to, 1.8h is stirred, it is molten to obtain third mixing
Liquid；
D, above-mentioned third mixed solution is put into the stainless steel autoclave with polytetrafluoroethyllining lining, is heated to 138
DEG C, pressure 3bar, stir 2.5h after filtering to get.
Embodiment 5:
A kind of preparation method of phosphorus doping self-cleaning list silver LOW-E glass the following steps are included:
A, phosphors coating titania coextruded film layer: with rolling method by 5% p-doped TiO2Solution is coated to the of thickness 8mm
On any side surface of one glass matrix, the phosphorus titania coextruded film layer that coating film thickness is 95nm is put into annealing furnace after coating
Middle tempering obtains the self-cleaning glass of tempering；
B, above-mentioned self-cleaning glass is not coated with clad can cleaning, is sent into magnetron sputtering machine after cleaning and successively carries out magnetic control
Sputtering；
C, plating sets the first Si3N4Film layer: being sputtered with AC power source, Ar, N2As sputter gas, magnetron sputtering sial target Si:
Al=92:8 (wt%), Ar, N2Gas flow 400SCCM:600SCCM, magnetron-sputtered film thickness are the first Si of 20nm3N4Film layer；
D, plating sets AZO film layer: being sputtered with AC power source, Ar, O2As sputter gas, magnetron sputtering Al-Doped ZnO target
ZnO:Al=92:8 (wt%), Ar, O2Gas flow 1000SCCM:40SCCM, magnetron-sputtered film thickness are the AZO film layer of 400nm；
E, plating sets Ag film layer: being sputtered with DC power supply, Ar is as sputter gas, gas flow 540SCCM, magnetron sputtering film
Thickness is the Ag film layer of 8.5nm；
F, plating sets NiCr film layer: being sputtered with DC power supply, Ar is as sputter gas, gas flow 500SCCM, magnetron sputtering
Film thickness is the NiCr film layer of 5nm；
G, plating sets the 2nd Si3N4Film layer: being sputtered with AC power source, Ar, N2As sputter gas, magnetron sputtering sial target Si:
Al=92:8 (wt%), Ar, N2Gas flow 400SCCM:600SCCM, magnetron-sputtered film thickness are the 2nd Si of 50nm3N4Film layer,
Obtain single layer phosphorus doping self-cleaning list silver LOW-E glass；
H, the single layer phosphorus doping self-cleaning list silver LOW-E glass plating processing synthesis: is equipped with the first Si3N4Film layer,
The AZO film layer, the Ag film layer, the NiCr film layer, the 2nd Si3N4The one side of film layer, the second glass with thickness 10mm
Glass matrix, which is separated out after hollow sealing chamber, to carry out processing synthesis and becomes hollow glass, both.
5% p-doped TiO described in above-mentioned steps A2The preparation method of solution includes the following steps:
A, 55ml butyl titanate is dissolved in 200ml dehydrated alcohol, 26mlH2O2In, 25min is stirred, is instilled while stirring
40ml deionized water obtains the first mixed solution；
B, 16ml acetylacetone,2,4-pentanedione, 20mlHNO are added in above-mentioned first mixed solution3, 48 DEG C are heated to, 28min is stirred,
Obtain the second mixed solution；
C, 12mlH is instilled in above-mentioned second mixed solution3PO4, 75 DEG C are heated to, 1.5h is stirred, it is molten to obtain third mixing
Liquid；
D, above-mentioned third mixed solution is put into the stainless steel autoclave with polytetrafluoroethyllining lining, is heated to 140
DEG C, pressure 4bar, stir 1.8h after filtering to get.
Embodiment 6:
A kind of preparation method of phosphorus doping self-cleaning list silver LOW-E glass the following steps are included:
A, phosphors coating titania coextruded film layer: with rolling method by 5% p-doped TiO2Solution is coated to the of thickness 8mm
On any side surface of one glass matrix, the phosphorus titania coextruded film layer that coating film thickness is 100nm is put into annealing furnace after coating
Middle tempering obtains the self-cleaning glass of tempering；
B, above-mentioned self-cleaning glass is not coated with clad can cleaning, is sent into magnetron sputtering machine after cleaning and successively carries out magnetic control
Sputtering；
C, plating sets the first Si3N4Film layer: being sputtered with AC power source, Ar, N2As sputter gas, magnetron sputtering sial target Si:
Al=92:8 (wt%), Ar, N2Gas flow 400SCCM:600SCCM, magnetron-sputtered film thickness are the first Si of 35nm3N4Film layer；
D, plating sets AZO film layer: being sputtered with AC power source, Ar, O2As sputter gas, magnetron sputtering Al-Doped ZnO target
ZnO:Al=92:8 (wt%), Ar, O2Gas flow 1000SCCM:40SCCM, magnetron-sputtered film thickness are the AZO film layer of 450nm；
E, plating sets Ag film layer: being sputtered with DC power supply, Ar is as sputter gas, gas flow 520SCCM, magnetron sputtering film
Thickness is the Ag film layer of 9.5nm；
F, plating sets NiCr film layer: being sputtered with DC power supply, Ar is as sputter gas, gas flow 540SCCM, magnetron sputtering
Film thickness is the NiCr film layer of 4nm；
G, plating sets the 2nd Si3N4Film layer: being sputtered with AC power source, Ar, N2As sputter gas, magnetron sputtering sial target Si:
Al=92:8 (wt%), Ar, N2Gas flow 400SCCM:600SCCM, magnetron-sputtered film thickness are the 2nd Si of 70nm3N4Film layer,
Obtain single layer phosphorus doping self-cleaning list silver LOW-E glass；
H, the single layer phosphorus doping self-cleaning list silver LOW-E glass plating processing synthesis: is equipped with the first Si3N4Film layer,
The AZO film layer, the Ag film layer, the NiCr film layer, the 2nd Si3N4The one side of film layer, the second glass with thickness 8mm
Glass matrix, which is separated out after hollow sealing chamber, to carry out processing synthesis and becomes hollow glass, both.
5% p-doped TiO described in above-mentioned steps A2The preparation method of solution includes the following steps:
A, 40ml butyl titanate is dissolved in 210ml dehydrated alcohol, 22mlH2O2In, 30min is stirred, is instilled while stirring
45ml deionized water obtains the first mixed solution；
B, 20ml acetylacetone,2,4-pentanedione, 24mlHNO are added in above-mentioned first mixed solution3, 50 DEG C are heated to, 25min is stirred,
Obtain the second mixed solution；
C, 6mlH is instilled in above-mentioned second mixed solution3PO4, 70 DEG C are heated to, 2.4h is stirred, obtains third mixed solution；
D, above-mentioned third mixed solution is put into the stainless steel autoclave with polytetrafluoroethyllining lining, is heated to 136
DEG C, pressure 3.5bar, stir 2.2h after filtering to get.
Comparative example 1
It is identical as 1 preparation method step of embodiment, but use the pure TiO undoped with phosphorus25% mixes in solution alternative steps A
Phosphorus TiO2Solution, to coat pure TiO2Film layer.
Comparative example 2
It is identical as 3 preparation step of embodiment, but use the pure TiO undoped with phosphorus25% p-doped TiO in solution alternative steps A2
Solution, to coat pure TiO2Film layer.
Table 1: the film layer of Examples 1 to 6 and comparative example 1~2 forms
Table 2: 5% p-doped TiO in Examples 1 to 6 step A2The proportion of solution
By product obtained by Examples 1 to 6 and comparative example 1~2, transmission of visible light, infrared transmittivity, biography are carried out respectively
Hot coefficient, shading coefficient, radiance optical performance test, while contact angle test is carried out, test result is as shown in table 3.
The measurement method of contact angle, includes the following steps:
A, sample to be tested successively is cleaned with distilled water, dehydrated alcohol, acetone, distilled water, and dry；
B, sample to be tested is put into Photoreactor and irradiates 1h；
C, sample to be tested is taken out, is placed on contact angle instrument (causing good ZJIA, ZJ-SDC-200) test sample to water
Contact angle.
Table 3: Examples 1 to 6 and 1~2 the performance test results of comparative example
It is low obtained by the embodiment of the present application by 3 test result of table it is found that Examples 1 to 6 is compared with comparative example 1~2
The transmission of visible light ﹥ 68% of radiant glass, and the pure TiO of comparative example2Obtained low emissivity glass is then respectively 45% He
52%, illustrate that the application has higher transmission of visible light, while in the application test result, infrared transmittivity ﹤ 19%, passing
Hot coefficient ﹤ 1.68 [W/ (㎡ K)], shading coefficient ﹤ 0.48, radiance ﹤ 0.086, are superior to the test data of comparative example, have
The characteristics of high visible light transmissivity, low-E, low infrared transmittivity, low heat transfer coefficient and low shading coefficient, allows visible
Light well penetrates the incoming interior of glass, enhances daylighting effect, while stopping from outdoor far-infrared thermal radiation.
Hydrophily is the important indicator of self-cleaning glass, is generally indicated with contact angle, can be intuitively anti-by contact angle
The quality for reflecting self-cleaning net effect, by 3 experimental result of table it is found that the application p-doped TiO2Obtained low emissivity glass, contact
4.9 ° of angle ﹤, and pure TiO2Obtained low emissivity glass, contact angle are 8.4 ° and 8.6 °.It may thus be appreciated that the application has more
Good self-cleaning net effect, has the self-cleaning net effect responded in 380~780nm of visible wavelength range, it is clear can to reduce cladding glass
Wash number.
Claims (10)
1. a kind of phosphorus doping self-cleaning list silver LOW-E glass, including the first glass substrate (1), the second glass matrix (2) and set
In hollow sealing chamber (3) between the two, it is characterised in that: first glass substrate (1) include the first glass matrix (11),
Set on first glass matrix (11) far from the phosphorus titania coextruded film layer (12) on hollow sealing chamber (3) face with
And successively plating is set to first Si of first glass matrix (11) on hollow sealing chamber (3) face3N4Film layer (13),
AZO film layer (14), Ag film layer (15), NiCr film layer (16), the 2nd Si3N4Film layer (17).
2. a kind of phosphorus doping self-cleaning list silver LOW-E glass according to claim 1, it is characterised in that: the phosphorus dioxy
Change titanium coextruded film layer (12) 90~110nm of film thickness.
3. a kind of phosphorus doping self-cleaning list silver LOW-E glass according to claim 1, it is characterised in that: described first
Si3N4Film layer (13) 20~45nm of film thickness.
4. a kind of phosphorus doping self-cleaning list silver LOW-E glass according to claim 1, it is characterised in that: the AZO film layer
(14) 300~500nm of film thickness.
5. a kind of phosphorus doping self-cleaning list silver LOW-E glass according to claim 1, it is characterised in that: the Ag film layer
(15) 8~10nm of film thickness.
6. a kind of phosphorus doping self-cleaning list silver LOW-E glass according to claim 1, it is characterised in that: the NiCr film
Layer (16) 3~5nm of film thickness.
7. a kind of phosphorus doping self-cleaning list silver LOW-E glass according to claim 1, it is characterised in that: described second
Si3N4Film layer (17) 50~85nm of film thickness.
8. a kind of phosphorus doping self-cleaning list silver LOW-E glass according to claim 1, it is characterised in that: first glass
Glass matrix (11) and second glass matrix (2) are the float glass of 4~10mm of thickness.
9. a kind of preparation method of phosphorus doping self-cleaning list silver LOW-E glass, it is characterised in that the following steps are included:
A, phosphors coating titania coextruded film layer: with rolling method by 5% p-doped TiO2Solution is coated to the of 4~10mm of thickness
On any side surface of one glass matrix, the phosphorus titania coextruded film layer that coating film thickness is 90~110nm is put into steel after coating
Change tempering in furnace, obtains the self-cleaning glass of tempering；
B, above-mentioned self-cleaning glass is not coated with clad can cleaning, successively carries out magnetic control in feeding magnetron sputtering machine after cleaning and splashes
It penetrates；
C, plating sets the first Si3N4Film layer: being sputtered with AC power source, Ar, N2As sputter gas, magnetron sputtering sial target Si:Al=
92:8 (wt%), Ar, N2Gas flow 400SCCM:600SCCM, magnetron-sputtered film thickness are the first Si of 20~45nm3N4Film layer；
D, plating sets AZO film layer: being sputtered with AC power source, Ar, O2As sputter gas, magnetron sputtering Al-Doped ZnO target ZnO:Al
=92:8 (wt%), Ar, O2Gas flow 1000SCCM:40SCCM, magnetron-sputtered film thickness are the AZO film layer of 300~500nm；
E, plating sets Ag film layer: being sputtered with DC power supply, Ar is as sputter gas, 500~550SCCM of gas flow, magnetron sputtering
Film thickness is the Ag film layer of 8~10nm；
F, plating sets NiCr film layer: being sputtered with DC power supply, Ar is splashed as sputter gas, 500~550SCCM of gas flow, magnetic control
Penetrate the NiCr film layer that film thickness is 3~5nm；
G, plating sets the 2nd Si3N4Film layer: being sputtered with AC power source, Ar, N2As sputter gas, magnetron sputtering sial target Si:Al=
92:8 (wt%), Ar, N2Gas flow 400SCCM:600SCCM, magnetron-sputtered film thickness are the 2nd Si of 50~85nm3N4Film layer,
Obtain single layer phosphorus doping self-cleaning list silver LOW-E glass；
H, the single layer phosphorus doping self-cleaning list silver LOW-E glass plating processing synthesis: is set into the first Si3N4It is film layer, described
AZO film layer, the Ag film layer, the NiCr film layer, the 2nd Si3N4The one side of film layer, the second glass with 4~10mm of thickness
Glass matrix, which is separated out after hollow sealing chamber, to carry out processing synthesis and becomes hollow glass, both.
10. a kind of preparation method of phosphorus doping self-cleaning list silver LOW-E glass according to claim 9, it is characterised in that:
5% p-doped TiO described in step A2The preparation method of solution includes the following steps:
A, 30~100ml butyl titanate is dissolved in 190~210ml dehydrated alcohol, 20~30mlH2O2In, stirring 20~
40min instills 30~50ml deionized water while stirring, obtains the first mixed solution；
B, 10~20ml acetylacetone,2,4-pentanedione, 20~30mlHNO are added in above-mentioned first mixed solution3, 30~50 DEG C are heated to, is stirred
20~40min is mixed, the second mixed solution is obtained；
C, 6~20mlH is instilled in above-mentioned second mixed solution3PO4, 70~90 DEG C are heated to, 1.5~2.5h is stirred, obtains third
Mixed solution；
D, above-mentioned third mixed solution is put into the stainless steel autoclave with polytetrafluoroethyllining lining, is heated to 130~140
DEG C, 3~4bar of pressure, stir 1.5~2.5h after filtering to get.
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